JP2014514449A - Tubular target with protective device - Google Patents

Tubular target with protective device Download PDF

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JP2014514449A
JP2014514449A JP2014502951A JP2014502951A JP2014514449A JP 2014514449 A JP2014514449 A JP 2014514449A JP 2014502951 A JP2014502951 A JP 2014502951A JP 2014502951 A JP2014502951 A JP 2014502951A JP 2014514449 A JP2014514449 A JP 2014514449A
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tubular target
protective device
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molybdenum
polymer
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JP2014514449A5 (en
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リンケ、クリスティアン
ズリーク、マンフレート
カトライン、マルティン
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プランゼー エスエー
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/342—Hollow targets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/3426—Material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3488—Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
    • H01J37/3491—Manufacturing of targets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3488—Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
    • H01J37/3497—Temperature of target

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  • Chemical & Material Sciences (AREA)
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  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Electrodes Of Semiconductors (AREA)

Abstract

本発明は、モリブデン又はモリブデン合金からなり、少なくとも一定の領域で冷媒と接触する内側表面（３）を備え、内側表面（３）の少なくとも一定の領域が少なくとも１つの保護装置（４）により冷媒（４）から分離されている、バッキングチューブを有しない陰極スパッタリング用管状ターゲット（１）に関する。保護装置（４）は、例えばポリマー層として設計可能である。管状ターゲット（１）は、卓越した長時間耐性を有する。
【選択図】図１The present invention comprises an inner surface (3) made of molybdenum or a molybdenum alloy and in contact with the refrigerant in at least a certain region, wherein at least a certain region of the inner surface (3) is cooled by at least one protective device (4) ( It relates to a tubular target (1) for cathode sputtering that does not have a backing tube and is separated from 4). The protective device (4) can be designed, for example, as a polymer layer. The tubular target (1) has excellent long-term resistance.
[Selection] Figure 1

Description

本発明は、スパッタ表面と、少なくとも部分的に冷媒と接触させられている内側表面とを、備える、モリブデン又は少なくとも５０原子％のモリブデン含有量を有するモリブデン合金からなる、陰極スパッタリング用のバッキングチューブを有しない管状ターゲットに関する。   The present invention provides a backing tube for cathode sputtering comprising a molybdenum surface or a molybdenum alloy having a molybdenum content of at least 50 atomic%, comprising a sputter surface and an inner surface that is at least partially in contact with a coolant. It relates to a tubular target that does not have.

純モリブデン及びモリブデン合金、例えばＭｏ−Ｎａ、からなる管状ターゲットは、Ｃｕ（Ｉｎx、Ｇａ1-x）（Ｓｅy、Ｓ1-y）2（Ｇａ：ＣＩＧＳ付き、Ｇａ：ＣＩＳなし）をベースとする薄膜太陽電池又はＴＦＴ−ＬＣＤ用の薄膜トランジスタの製造時等における、陰極スパッタリング、例えばマグネトロンスパッタリング、によるモリブデン含有層の堆積に使用される。この場合、モリブデン含有層は、数ｎｍから数μｍの厚さを有する。スパッタリングに必要な出発材料（陰極）は、スパッタリングターゲットと呼ばれ、塗被設備の形態に応じて、平板又は管の形で使用される。管状ターゲットとも呼ばれる管状スパッタリングターゲットは、操作中に、ターゲットの内部に配置された固定磁石系又は可動磁石系の周りを回転させられる。平板状のスパッタリングターゲットに比べて、管状スパッタリングターゲットは、材料の均一な除去と従って高い材料収率とが達成される利点を有する。特に製造が複雑な高価な材料については、管状スパッタリングターゲットが勝っている。セラミック及び脆性材料では、管状ターゲットは、少なくとも２分割され、管状ターゲットの保持及び移動に必要な力が脆性の、従って破損しやすい、スパッタ材料に作用しないようにされている。この場合、スパッタ材料からなる管又は複数の管片は、例えば非磁性鋼又はチタンからなる、バッキングチューブと接合される。接合技術として、低融点の半田、例えばインジウム又はインジウム合金、を使用する半田付け法が用いられている。 Pure molybdenum and molybdenum alloys, for example, Mo-Na, tubular target formed from, Cu (In x, Ga 1 -x) (Se y, S 1-y) 2 (Ga: with CIGS, Ga: no CIS) based The film is used for depositing a molybdenum-containing layer by cathode sputtering, for example, magnetron sputtering, in the production of a thin film solar cell or TFT-LCD thin film transistor. In this case, the molybdenum-containing layer has a thickness of several nm to several μm. The starting material (cathode) necessary for sputtering is called a sputtering target and is used in the form of a flat plate or a tube depending on the form of the coating equipment. Tubular sputtering targets, also called tubular targets, are rotated around a fixed or movable magnet system disposed within the target during operation. Compared to flat sputtering targets, tubular sputtering targets have the advantage that a uniform removal of the material and thus a high material yield is achieved. Especially for expensive materials that are complex to manufacture, tubular sputtering targets are superior. In ceramic and brittle materials, the tubular target is divided into at least two parts so that the force required to hold and move the tubular target does not act on the sputtered material, which is brittle and therefore prone to breakage. In this case, the tube or the plurality of tube pieces made of the sputtered material is joined to a backing tube made of nonmagnetic steel or titanium, for example. As a joining technique, a soldering method using a low melting point solder such as indium or an indium alloy is used.

スパッタリングの際に用いられるエネルギーの７５％超は、熱としてスパッタリングターゲットに入る。スパッタリングターゲットの表面上への高エネルギーイオンの衝撃により発生する熱エネルギーは、スパッタリングターゲット材料及び／又は半田材料の過熱を防ぐために、十分に効果的に、放散する必要がある。それ故、スパッタリングターゲットの冷却は、重要な意味を持つ。管状ターゲットの場合、スパッタリングターゲットの内側表面が、全面的に又は一定の領域において、冷媒の貫流により冷却される。この場合、冷媒は、管状ターゲットの形態に応じて、スパッタ材料に直接接触させられるか又はバッキングチューブに接触させられる。   More than 75% of the energy used during sputtering enters the sputtering target as heat. The thermal energy generated by the bombardment of high energy ions on the surface of the sputtering target must be dissipated sufficiently effectively to prevent overheating of the sputtering target material and / or solder material. Therefore, cooling the sputtering target is important. In the case of a tubular target, the inner surface of the sputtering target is cooled entirely or in certain areas by the flow of coolant. In this case, the refrigerant is brought into direct contact with the sputtered material or brought into contact with the backing tube, depending on the form of the tubular target.

モリブデン又はモリブデン合金製の管状ターゲットは、広くバッキングチューブとともに使用されている。この場合の欠点は、スパッタ材料とバッキングチューブとの接合に労力を要することだけではなく、密実なバッキングチューブ及び半田材料により熱拡散が妨げられることである。例えば鋼は、モリブデンに比して相当程度、熱伝導特性が劣っている。   Tubular targets made of molybdenum or molybdenum alloys are widely used with backing tubes. The disadvantage in this case is not only that labor is required for joining the sputtered material and the backing tube, but also that heat diffusion is hindered by the dense backing tube and solder material. For example, steel is inferior in heat conductivity to a considerable extent compared to molybdenum.

モリブデン又はモリブデン合金製の管状ターゲットがバッキングチューブなしで作られると、冷媒とターゲット材料との直接的な接触が生じる。モリブデン及びモリブデン合金は、通常の冷媒の長時間の作用を受けると、腐食する。この場合の腐食速度は、冷媒の組成及び種類並びに使用条件に応じて、１年に１０分の数ミリメートルに達する。冷媒との接触により生じるモリブデンの溶解及びこの場合に発生する腐食生成物（主としてモリブデン酸塩又は例えば銅との混合モリブデン酸塩）により、冷媒の特性が変化する。例えば、冷媒のｐＨ値が著しく低下し、それとともに冷却循環路において使用されるほかの材料（例えば銅、真鍮、特殊鋼）が著しく腐食作用を受ける。冷却循環路におけるモリブデン及びほかの材料の腐食は、有機又は無機抑制剤の冷媒への添加により抑制されるが、完全に防止することはできない。モリブデン用の腐食抑制剤は、例えば特許文献１に記載されている。冷媒の状態の定期的監視及び場合によって必要な添加物の補充は、更に設備経費を高めることになる。   When a tubular target made of molybdenum or molybdenum alloy is made without a backing tube, direct contact between the refrigerant and the target material occurs. Molybdenum and molybdenum alloys corrode when subjected to the long-term action of ordinary refrigerants. The corrosion rate in this case reaches a few tenths of a millimeter per year, depending on the composition and type of refrigerant and the conditions of use. The characteristics of the refrigerant change due to the dissolution of molybdenum caused by contact with the refrigerant and the corrosion products generated in this case (mainly molybdate or a mixed molybdate with copper, for example). For example, the pH value of the refrigerant is significantly reduced, and other materials used in the cooling circuit (for example, copper, brass, special steel) are significantly corroded. Corrosion of molybdenum and other materials in the cooling circuit is suppressed by the addition of organic or inorganic inhibitors to the refrigerant, but cannot be completely prevented. A corrosion inhibitor for molybdenum is described in Patent Document 1, for example. Regular monitoring of refrigerant status and replenishment of necessary additives may further increase equipment costs.

使用される冷媒の特性の一覧例を表１にまとめる。

Figure 2014514449
Table 1 summarizes examples of characteristics of refrigerants used.
Figure 2014514449

更に考慮しなければならないことは、モリブデンの原料価格が極めて高いことである。モリブデン製の使用済みスパッタリングターゲットは、通常はリサイクルされずに、コンパクトな形で鋼及び超合金の製造用の合金金属として使用される。（ほかの金属の混入のない）単一品のスクラップは、通常の鋼合金にとっては異種である元素を含むＭｏスクラップよりも明らかに高い価格になる。それ故、バッキングチューブを備えたモリブデン管ターゲットは、まず半田付けを解き、通常は鋼合金にとって異種である半田材料を、労力を掛けて、除去する必要がある。   A further consideration is that the raw material price of molybdenum is very high. Spent sputtering targets made of molybdenum are not normally recycled but are used in compact form as alloy metals for the production of steel and superalloys. A single piece of scrap (without any other metal contamination) is clearly more expensive than a Mo scrap containing elements that are dissimilar to ordinary steel alloys. Therefore, a molybdenum tube target with a backing tube must first be unsoldered and remove the solder material that is usually dissimilar to the steel alloy with effort.

米国特許第４７１９０３５号明細書US Pat. No. 4,719,035

それ故、本発明の課題は、先行技術の項で述べたような欠点を持たないモリブデン又はモリブデン合金製の管状ターゲットを提供することにある。この点に関して特に強調すべきことは、熱放散が十分に保証され、管状ターゲットの使用期間全体に亘って腐食をできる限り回避し、そして、使用済みスパッタリングターゲットが鋼工業用の合金材料として容易に使用できるようにすることである。   The object of the present invention is therefore to provide a tubular target made of molybdenum or a molybdenum alloy which does not have the disadvantages mentioned in the prior art section. What should be particularly emphasized in this regard is that heat dissipation is sufficiently ensured, corrosion is avoided as much as possible throughout the lifetime of the tubular target, and the used sputtering target is easily used as an alloy material for the steel industry. Is to be able to use it.

この課題は、独立請求項の特徴部分により解決される。本発明の実施により、腐食は確実に避けられ、熱放散が許容できないほど悪くなることはない。更に、使用済み管状ターゲットは、労力の掛かる分離や洗浄なしに、鋼製造用合金スクラップとして使用できる。何故なら、保護装置のモリブデン成分量は、僅かであるからである。   This problem is solved by the features of the independent claims. By implementing the present invention, corrosion is reliably avoided and heat dissipation is not unacceptably worse. Furthermore, the used tubular target can be used as an alloy scrap for steel production without labor intensive separation or cleaning. This is because the amount of molybdenum component in the protective device is very small.

図１は、本発明による管状ターゲットの概略斜視図である。FIG. 1 is a schematic perspective view of a tubular target according to the present invention.

管状ターゲットは、純モリブデン又はモリブデン合金からなる。この場合、モリブデン合金とは、モリブデン含有量が５０原子％を超える全てのモリブデン含有材料を指す。以下の記載でモリブデンについて言及するときは、常に純モリブデンとモリブデン含有量が５０原子％を超える全てのモリブデン含有材料とを含むものとする。管状ターゲットは、バッキングチューブなしで形成される。この場合、「バッキングチューブなし」とは、バッキングチューブが全く使用されないことを意味する。モリブデン管状ターゲットは、それ故、スパッタ設備の保持系又は端末ブロックに直接接合される。スパッタ表面とは、管状ターゲットの外側表面のことを言う。内側表面は、管状ターゲットの内壁に相当する。内側表面の少なくとも一部の領域は、少なくとも１つの保護装置により、冷媒から分離される。ターゲット材料と保護装置との面接触が生じると有利である。更に、冷媒と接触する全ての内側表面が、少なくとも１つの保護装置により、冷媒から分離されると有利である。保護装置が（半径方向に測定して）０．０００５ｍｍ〜１ｍｍの厚さを有すると有利である。特に有利なのは、保護装置が（半径方向に測定して）０．０００５ｍｍ〜０．１ｍｍの厚さを有することである。保護装置の熱伝導率が１Ｗ／ｍ．Ｋ未満であれば、保護装置の厚さは、０．０００５ｍｍ〜０．５ｍｍが好適である。更に、保護装置が単層又は複層であれば有利である。層の付着を改良するためには、保護装置の取り付け前に、管の内側表面を前処理、例えば脱脂又は粗面化、すると有利である。更に有利な実施形態は、保護装置が薄壁の膜又は薄壁の管の形をとり、加圧された冷媒の作用下で、管状ターゲットの内側表面に継ぎ目なく当接することである。この場合、薄壁とは１ｍｍまでの範囲の厚さのものを言う。保護装置は、少なくともポリマー、金属、セラミック及びガラスからなる群から選ばれる１つの材料からなると有利である。好適な金属は、例えばニッケルであり、これは、化学的ニッケルメッキにより簡単に取り付けることができる。セラミック材料では、モリブデン窒化物が挙げられるが、これはモリブデン管の窒化により簡単に製造できる。ガラスからなる層では、ケイ素酸化物をベースとする系が特に適している。   The tubular target is made of pure molybdenum or a molybdenum alloy. In this case, the molybdenum alloy refers to all molybdenum-containing materials whose molybdenum content exceeds 50 atomic%. References to molybdenum in the following description always include pure molybdenum and all molybdenum-containing materials with a molybdenum content greater than 50 atomic percent. The tubular target is formed without a backing tube. In this case, “no backing tube” means that no backing tube is used. The molybdenum tubular target is therefore directly joined to the holding system or terminal block of the sputtering equipment. The sputter surface refers to the outer surface of the tubular target. The inner surface corresponds to the inner wall of the tubular target. At least a portion of the inner surface is separated from the refrigerant by at least one protective device. It is advantageous if surface contact between the target material and the protective device occurs. Furthermore, it is advantageous if all inner surfaces in contact with the refrigerant are separated from the refrigerant by at least one protective device. It is advantageous if the protective device has a thickness (measured in the radial direction) of 0.0005 mm to 1 mm. It is particularly advantageous that the protective device has a thickness of 0.0005 mm to 0.1 mm (measured in the radial direction). The thermal conductivity of the protective device is 1 W / m. If it is less than K, 0.0005 mm-0.5 mm are suitable for the thickness of a protective device. Furthermore, it is advantageous if the protective device is a single layer or multiple layers. In order to improve the adhesion of the layers, it is advantageous if the inner surface of the tube is pretreated, for example degreased or roughened, before the protective device is installed. A further advantageous embodiment is that the protective device takes the form of a thin-walled membrane or a thin-walled tube and seamlessly abuts the inner surface of the tubular target under the action of a pressurized refrigerant. In this case, the thin wall means one having a thickness in the range of up to 1 mm. The protective device is advantageously made of at least one material selected from the group consisting of polymer, metal, ceramic and glass. A suitable metal is, for example, nickel, which can be easily attached by chemical nickel plating. Ceramic materials include molybdenum nitride, which can be easily manufactured by nitriding a molybdenum tube. For layers made of glass, systems based on silicon oxide are particularly suitable.

更に、鋼製造にとって問題のない材料としては、例えばポリマーのように、その成分（炭素）が一方では鋼の全炭素含有量に関して問題のない添加材料であり他方では鋼製造の際に気体の形（窒素・水素・塩素・フッ素等）で消失する材料が、選ばれる。保護装置がセラミック又はガラスから成る場合には、鋼製造時にこれらの成分はスラグとして析出される。   Furthermore, as a material that is not problematic for steel production, for example, its component (carbon) is an additive material that is not problematic with respect to the total carbon content of the steel, on the one hand, and on the other hand in the form of gas during steel production. Materials that disappear with (nitrogen, hydrogen, chlorine, fluorine, etc.) are selected. If the protective device is made of ceramic or glass, these components are deposited as slag during steel production.

製造コスト及びリサイクル性を考慮すると、保護装置が少なくとも１つのポリマーを含有してなると有利である。ポリマーが０．５Ｗ／ｍ．Ｋを超える、特に１Ｗ／ｍ．Ｋを超える、熱伝導率を有すると特に有利である。電気伝導性も管状ターゲットの使用特性に有利に作用する。熱及び／又は電気伝導性は、例えば、ポリマーが１つ又は複数の伝導性充填材を備えていれば得られる。好適な充填材としては、セラミック、グラファイト及び金属からなる群から選ばれる材料が挙げられる。特に好適な充填材は、Ｃｕ、Ａｌ、Ｓｉ、Ｚｎ、Ｍｏ、Ｗ、例えばＡｌ2Ｏ3のような酸化物、例えばＡｌＮ、ＴｉＮ、ＢＮ、ＭｏＮ又はＳｉＮのような窒化物、例えばＳｉＣ、ＴｉＣ又はＷＣのようなカーバイド、及び、グラファイトである。 In view of production costs and recyclability, it is advantageous if the protective device comprises at least one polymer. Polymer was 0.5 W / m. K, in particular 1 W / m. It is particularly advantageous to have a thermal conductivity exceeding K. Electrical conductivity also has an advantageous effect on the usage characteristics of the tubular target. Thermal and / or electrical conductivity can be obtained, for example, if the polymer comprises one or more conductive fillers. Suitable fillers include materials selected from the group consisting of ceramic, graphite and metal. Particularly suitable fillers are Cu, Al, Si, Zn, Mo, W, oxides such as Al 2 O 3 , eg nitrides such as AlN, TiN, BN, MoN or SiN, eg SiC, TiC. Or carbide such as WC and graphite.

更に、保護装置が少なくとも１つのポリマーからなると有利である。非充填及び充填状態において特に好適なポリマーは、エポキシ樹脂、ポリエチレン、ポリプロピレン、ポリウレタン、ポリ塩化ビニル、ポリエステル、ビニルエステル及びフッ素化エラストマーからなる群から選ばれるポリマーである。   Furthermore, it is advantageous if the protective device consists of at least one polymer. Particularly preferred polymers in the unfilled and filled state are polymers selected from the group consisting of epoxy resins, polyethylene, polypropylene, polyurethane, polyvinyl chloride, polyesters, vinyl esters and fluorinated elastomers.

保護装置は、湿式塗布、塗装、噴霧又は箔の貼り付けにより載置し又は取り付けると有利である。   The protective device is advantageously placed or attached by wet application, painting, spraying or foil application.

しかし、また、ほかの塗被方法、例えば化学的気相析出（ＣＶＤ）、熱噴霧、低温噴霧、ゾル・ゲル塗被法、メッキ、陰極スパッタリング（ＰＶＤ）、電気メッキ、化学的及び電気化学的プロセス、焼結、拡散塗被、擦り付け、又はバックキャスティングも適している。   However, other coating methods such as chemical vapor deposition (CVD), thermal spraying, low temperature spraying, sol-gel coating, plating, cathode sputtering (PVD), electroplating, chemical and electrochemical Process, sintering, diffusion coating, rubbing, or back casting is also suitable.

以下に本発明を実施例により説明する。   Hereinafter, the present invention will be described by way of examples.

図１は、スパッタ表面（２）、内側表面（３）及び保護装置（４）を備えた本発明による管状ターゲット（１）の概略斜視図を示す。   FIG. 1 shows a schematic perspective view of a tubular target (1) according to the invention with a sputter surface (2), an inner surface (3) and a protective device (4).

〔例１〕
１２５ｍｍの内径と１６５ｍｍの外径とを有し、スパッタ表面（２）を備えたモリブデン管（１）は、欧州特許出願公開第１９３７８６６号明細書に記載された製法で作られた。モリブデン管の塗被すべき内側表面（３）は、１，５００ｍｍの長さを有していた。塗被されるべき内側表面は、先ず、サンドブラストで粗面化された。続いての塗被は、粒径５０μｍのＡｌを７０容量％充填したエポキシ樹脂の塗付により行なわれた。保護装置（４）の層厚は、約３００μｍであった。 [Example 1]
A molybdenum tube (1) having an inner diameter of 125 mm and an outer diameter of 165 mm and provided with a sputter surface (2) was made by the process described in EP 1937866. The inner surface (3) to be coated of the molybdenum tube had a length of 1,500 mm. The inner surface to be coated was first roughened by sandblasting. Subsequent coating was performed by applying an epoxy resin filled with 70% by volume of Al having a particle size of 50 μm. The layer thickness of the protective device (4) was about 300 μm.

〔例２〕
直径１０ｍｍ及び長さ５０ｍｍの円筒状モリブデン試料の耐腐食性が、塗被されてない状態及び塗被された状態（例２ａ−２ｇ）で、曝露テストにより、試験された。サンプルは、この場合、種々の冷媒中において１６０時間の期間に亘り貯蔵され、サンプルの質量減少が測定された。冷媒浴は、実験期間中、マグネチックスターラーにより撹拌された。測定結果を表２に示した。Ｒで示したサンプル（参照サンプル）は、従来技術に相当する（塗被されていない）。例２ａから２ｇは、本発明による例である。 [Example 2]
The corrosion resistance of cylindrical molybdenum samples 10 mm in diameter and 50 mm in length was tested by an exposure test in the uncoated state and in the coated state (Examples 2a-2g). The sample was then stored in various refrigerants for a period of 160 hours and the mass loss of the sample was measured. The refrigerant bath was stirred by a magnetic stirrer during the experiment. The measurement results are shown in Table 2. The sample indicated by R (reference sample) corresponds to the prior art (not coated). Examples 2a to 2g are examples according to the invention.

〔例２ａ〕
塗被すべき表面は、サンドブラストで粗面化された。続いての塗被は、粒径５０μｍのＡｌを７０容量％充填したエポキシ樹脂の塗付により行なわれた。層厚は、約３００μｍであった。 [Example 2a]
The surface to be coated was roughened by sandblasting. Subsequent coating was performed by applying an epoxy resin filled with 70% by volume of Al having a particle size of 50 μm. The layer thickness was about 300 μm.

〔例２ｂ〕
塗被すべき表面は、サンドブラストで粗面化された。続いての塗被はアルキド樹脂塗料（ポリエステル）の湿式塗付により行なわれ、空気中で乾燥された。層厚は、約１００μｍであった。 [Example 2b]
The surface to be coated was roughened by sandblasting. Subsequent coating was performed by wet coating of an alkyd resin paint (polyester) and dried in air. The layer thickness was about 100 μm.

〔例２ｃ〕
塗被すべき表面は、サンドブラストで粗面化された。続いての塗被は粒径５０μｍのＡｌ2Ｏ3を７０容量％充填したエポキシ樹脂の塗付により行なわれた。層厚は、約３００μｍであった。 [Example 2c]
The surface to be coated was roughened by sandblasting. Subsequent coating was performed by applying an epoxy resin filled with 70% by volume of Al 2 O 3 having a particle size of 50 μm. The layer thickness was about 300 μm.

〔例２ｄ〕
塗被すべき表面は、酸洗いにより洗浄脱脂された。続いての塗被は、ポリウレタン化合物の粉末噴霧により行なわれた。層厚は、約５００μｍであった。 [Example 2d]
The surface to be coated was washed and degreased by pickling. Subsequent coating was performed by powder spraying of the polyurethane compound. The layer thickness was about 500 μm.

〔例２ｅ〕
塗被すべき表面は、酸洗いにより洗浄脱脂された。通常のメッキ化学法（硫酸銅ベース）で厚さ１５μｍの銅層が析出された。 [Example 2e]
The surface to be coated was washed and degreased by pickling. A copper layer having a thickness of 15 μm was deposited by an ordinary plating chemical method (based on copper sulfate).

〔例２ｆ〕
塗被すべき表面は、サンドブラストで粗面化された。続いてＳｉＯ2をベースとするスラリーが塗布され、２００℃／６０ｍｉｎで熱処理された。 [Example 2f]
The surface to be coated was roughened by sandblasting. Subsequently, a slurry based on SiO 2 was applied and heat-treated at 200 ° C./60 min.

〔例２ｇ〕
塗被すべき表面は、サンドブラストで粗面化された。続いて厚さ２μｍのＴｉＮ層がＣＶＤにより適用された。 [Example 2g]
The surface to be coated was roughened by sandblasting. Subsequently, a 2 μm thick TiN layer was applied by CVD.

Figure 2014514449
Figure 2014514449

１ 管状ターゲット
２ スパッタ表面
３ 内側表面
４ 保護装置 DESCRIPTION OF SYMBOLS 1 Tubular target 2 Sputtering surface 3 Inner surface 4 Protection device

Claims (15)

モリブデン又は少なくとも５０原子％のモリブデン含有量を有するモリブデン合金からなり、スパッタ表面（２）と、少なくとも一定の領域で冷媒と接触する内側表面（３）とを、備えた陰極スパッタリング用のバッキングチューブのない管状ターゲット（１）において、前記内側表面（３）の少なくとも一定の領域が少なくとも１つの保護装置（４）により冷媒（４）から分離されていることを特徴とする管状ターゲット。   A backing tube for cathode sputtering comprising molybdenum or a molybdenum alloy having a molybdenum content of at least 50 atomic% and comprising a sputter surface (2) and an inner surface (3) in contact with a coolant in at least a certain area. Non-tubular target (1), characterized in that at least certain areas of the inner surface (3) are separated from the refrigerant (4) by at least one protective device (4). 前記保護装置（４）が前記内側表面（３）と面接触していることを特徴とする請求項１に記載の管状ターゲット。   Tubular target according to claim 1, characterized in that the protective device (4) is in surface contact with the inner surface (3). 前記保護装置（４）が０．０００５ｍｍ〜１ｍｍの厚さを有していることを特徴とする請求項１又は２に記載の管状ターゲット。   Tubular target according to claim 1 or 2, characterized in that the protective device (4) has a thickness of 0.0005 mm to 1 mm. 前記保護装置（４）が０．０００５ｍｍ〜０．１ｍｍの厚さを有していることを特徴とする請求項３に記載の管状ターゲット。   The tubular target according to claim 3, characterized in that the protective device (4) has a thickness of 0.0005 mm to 0.1 mm. 前記保護装置（４）が単層又は複層であることを特徴とする請求項１〜４のいずれか１項に記載の管状ターゲット。   The tubular target according to any one of claims 1 to 4, wherein the protective device (4) is a single layer or multiple layers. 前記保護装置（４）が箔であることを特徴とする請求項１〜５のいずれか１項に記載の管状ターゲット。   The tubular target according to claim 1, wherein the protective device is a foil. 冷媒と接触している内側表面が、全て、少なくとも１つの保護装置（４）により冷媒から分離されていることを特徴とする請求項１〜６のいずれか１項に記載の管状ターゲット。   Tubular target according to any one of the preceding claims, characterized in that the inner surface in contact with the refrigerant is all separated from the refrigerant by at least one protective device (4). 前記保護装置（４）がポリマー、金属、セラミック及びガラスからなる群から選ばれる少なくとも１つの材料から成ることを特徴とする請求項１〜７の１つに記載の管状ターゲット。   Tubular target according to one of claims 1 to 7, characterized in that the protective device (4) is made of at least one material selected from the group consisting of polymers, metals, ceramics and glasses. 前記保護装置（４）が少なくとも１つのポリマーを含有してなることを特徴とする請求項１〜８のいずれか１項に記載の管状ターゲット。   The tubular target according to any one of claims 1 to 8, wherein the protective device (4) comprises at least one polymer. 前記ポリマーが伝熱性及び／又は導電性を有することを特徴とする請求項９に記載の管状ターゲット。   The tubular target according to claim 9, wherein the polymer has heat conductivity and / or conductivity. 前記ポリマーが充填材を含有してなることを特徴とする請求項９又は１０に記載の管状ターゲット。   The tubular target according to claim 9 or 10, wherein the polymer contains a filler. 前記充填材がセラミック、グラファイト及び金属からなる群から選ばれる少なくとも１つの材料からなることを特徴とする請求項１１に記載の管状ターゲット。   The tubular target according to claim 11, wherein the filler is made of at least one material selected from the group consisting of ceramic, graphite, and metal. 前記保護装置（４）が少なくとも１つのポリマーを含有して成ることを特徴とする請求項９〜１２のいずれか１項に記載の管状ターゲット。   13. Tubular target according to any one of claims 9 to 12, characterized in that the protective device (4) comprises at least one polymer. 前記ポリマーが、エポキシ樹脂、ポリエチレン、ポリプロピレン、ポリウレタン、ポリ塩化ビニル、ポリエステル、ビニルエステル及びフルオロエラストマからなる群から選ばれるポリマーであることを特徴とする請求項９〜１３のいずれか１項に記載の管状ターゲット。   14. The polymer according to claim 9, wherein the polymer is a polymer selected from the group consisting of epoxy resin, polyethylene, polypropylene, polyurethane, polyvinyl chloride, polyester, vinyl ester, and fluoroelastomer. Tubular target. 前記保護装置（４）が湿式塗布、噴霧及び箔の挿入からなる群から選ばれる１つのプロセスにより取り付けられることを特徴とする請求項１〜１４のいずれか１項に記載の管状ターゲットの製造方法。   15. The method of manufacturing a tubular target according to any one of claims 1 to 14, wherein the protective device (4) is attached by one process selected from the group consisting of wet coating, spraying and foil insertion. .
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AT12695U1 (en) 2012-10-15
CN103518002A (en) 2014-01-15
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WO2012135883A1 (en) 2012-10-11
US10978279B2 (en) 2021-04-13
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US20140027276A1 (en) 2014-01-30
JP6328550B2 (en) 2018-05-23

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